Category: 105-53-3

A common heterocyclic compound, 105-53-3, name is Diethyl malonate, molecular formula is C7H12O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 105-53-3.

General procedure: PhIO (550 mg, 2.5 mmol), Et3N¡¤5HF (800 mg, 4 mmol), and DCE (1 mL)were placed in a Teflon test tube. After stirring at r.t. for 15 min, the appropriate malonic ester 1 (1 mmol) and DCE (1 mL) were added. The test tube was sealed with a septum rubber and heated at 70 C for 24 h with stirring. The reaction mixture was neutralized with aq NaHCO3 and the product was extracted with CH2Cl2 (3 ¡Á 10 mL). The combined organic layers were washed with brine (20 mL), dried (Na2SO4), and concentrated under reduced pressure. The product was purified by column chromatography on silica gel with hexane-CH2Cl2 as eluent.

The synthetic route of Diethyl malonate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kitamura, Tsugio; Muta, Kensuke; Oyamada, Juzo; Synthesis; vol. 47; 20; (2015); p. 3241 – 3245;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 105-53-3, name is Diethyl malonate, molecular formula is C7H12O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 105-53-3

To a solution of diethyl malonate (3.2 g, 20 mmol) and anhydrous potassium carbonate powder (6.9 g, 50 mmol) in DMF (50.0 mL) was added 1,2-dibromoethane (4.136 g, 22 mmol). After stirring for 2 hrs, catalytic amount of TBAI (0.738 g, 2.0 mmol) was added and the mixture was continued to stir at room temperature for 8 hrs. The reaction mixture was filtered and the solid was washed with diethyl ether 3 times. The filtrate was diluted with water (200 mL) and extracted with diethyl ether (75 mL*4). The combined organic phases were washed with 70 mL of brine, dried over Na2SO4 and concentrated in vacuo. The residue was chromatographed with a short alumina column (1: 10 (v/v) EtOAc / n-hexane) to afford the desired compound as yellow oil (3.3 g, 88.7 %). 1H NMR (400MHz, CDCl3): delta 1.27 (m, J=6.8Hz, 6H), 1.42 (m, 4H), 4.18 (m, 4H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 105-53-3, its application will become more common.

Reference:
Patent; Sunshine Lake Pharma Co., Ltd.; Xi, Ning; XI, Ning; (152 pag.)EP2408300; (2016); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

A common heterocyclic compound, 105-53-3, name is Diethyl malonate, molecular formula is C7H12O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 105-53-3.

A solution of Malonate 2.2 (1 eq) and acid (trifluoroacetic acid) (0.1 eq.) was prepared in acetonitrile (5 volumes) and was added slowly at a rate such that the internal temperature never exceeded 25 C. (time of addition=10-15 minutes). The reaction was complete in two hours at room temperature and achieve an in-solution conversion of 76%

The synthetic route of Diethyl malonate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; OptMed, Inc.; Gondi, Vijaya Bhasker; Reid, John Gregory; US2013/197263; (2013); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics